CN114440554A - Device and method for producing high-purity oxygen - Google Patents

Device and method for producing high-purity oxygen Download PDF

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Publication number
CN114440554A
CN114440554A CN202210093413.3A CN202210093413A CN114440554A CN 114440554 A CN114440554 A CN 114440554A CN 202210093413 A CN202210093413 A CN 202210093413A CN 114440554 A CN114440554 A CN 114440554A
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nitrogen
oxygen
liquid
heat exchanger
liquid nitrogen
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CN114440554B (en
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陈志诚
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Zhongke Fuhai Hangzhou Gas Engineering Technology Co ltd
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Zhongke Fuhai Hangzhou Gas Engineering Technology Co ltd
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J5/00Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/02Processes or apparatus using separation by rectification in a single pressure main column system
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/50Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00Processes characterised by the type or other details of the feed stream
    • F25J2210/42Nitrogen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/04Recovery of liquid products
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/50Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F25J2215/56Ultra high purity oxygen, i.e. generally more than 99,9% O2
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00Processes or apparatus involving steps for the removal of impurities
    • F25J2220/52Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/12External refrigeration with liquid vaporising loop
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/42Quasi-closed internal or closed external nitrogen refrigeration cycle
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/90External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The invention relates to a device and a method for producing high purity oxygen, wherein the scheme comprises a buffer tank, a liquid nitrogen circulating channel and a cold box, wherein raw material oxygen is arranged in the buffer tank; the cold box is internally provided with a main heat exchanger, a rectifying tower, an auxiliary heat exchanger, an evaporator and a condenser; the buffer tank is sequentially communicated with the main heat exchanger, the rectifying tower and the auxiliary heat exchanger through an oxygen channel, and high-purity liquid oxygen is discharged through a high-purity liquid oxygen outlet pipeline; the liquid nitrogen circulation channel comprises a liquid nitrogen inlet pipeline positioned outside the cold box, a circulation pipeline partially positioned in the cold box, a vent pipe positioned outside the cold box and a nitrogen compressor, wherein the circulation pipeline is sequentially communicated with the auxiliary heat exchanger, the main heat exchanger, the nitrogen compressor, the main heat exchanger, the evaporator, the throttle valve, the condenser, the auxiliary heat exchanger and pipelines between the auxiliary heat exchanger and the main heat exchanger from the liquid nitrogen inlet pipeline. The method has the advantages of simple flow, low energy consumption, high pure oxygen recovery rate and complete independence from a krypton-xenon production system.

Description

Device and method for producing high-purity oxygen
Technical Field
The invention relates to the technical field of pure oxygen manufacturing, in particular to a device and a method for producing high-purity oxygen.
Background
At present, the production flow of high purity oxygen mainly adopts a cryogenic rectification method, and high boiling point components in oxygen are removed in advance in the production process, wherein the high boiling point components mainly comprise hydrocarbons such as methane, krypton, xenon, fluoride and the like. In order to remove the high boiling point components in the oxygen, the traditional method needs to arrange a corresponding rectifying tower, and the process has high energy consumption and large investment. In the process of extracting krypton-xenon from liquid oxygen, after oxygen is subjected to the processes of krypton-xenon preconcentration, methane removal and krypton-xenon secondary concentration, the oxygen discharged from the top of the krypton-xenon secondary concentration tower does not contain high-boiling-point components such as krypton, xenon, methane, nitrous oxide and the like. Therefore, the by-product oxygen is usually sent into a pipe network as common oxygen, and cannot be further processed to improve the added value, thereby causing waste.
In summary, an apparatus and a method for extracting high purity oxygen from oxygen or liquid oxygen, which is a byproduct after extracting krypton and xenon, are needed to solve the above technical problems.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a device and a method for producing high-purity oxygen, which have the advantages of simple process, low energy consumption and high extraction rate.
In order to realize the purpose of the invention, the invention adopts the following technical scheme: a device for producing high purity oxygen comprises a buffer tank with raw material oxygen arranged therein, a liquid nitrogen circulation channel and a cold box; the cold box is internally provided with a main heat exchanger, a rectifying tower, an auxiliary heat exchanger, an evaporator arranged at the bottom of the rectifying tower and a condenser arranged at the top of the rectifying tower;
the cold box is used for cooling all the components in the cold box so that all the components are at different temperatures, and the heat preservation is carried out among all the components by filling heat preservation materials;
the buffer tank is sequentially communicated with the main heat exchanger, the rectifying tower and the auxiliary heat exchanger through an oxygen channel, and high-purity liquid oxygen is discharged through a high-purity liquid oxygen outlet pipeline;
the liquid nitrogen circulation channel comprises a liquid nitrogen inlet pipeline positioned outside the cold box, a circulation pipeline partially positioned in the cold box, an emptying pipe positioned outside the cold box and a nitrogen compressor, wherein the circulation pipeline is sequentially communicated with the auxiliary heat exchanger, the main heat exchanger, the nitrogen compressor, the main heat exchanger, the evaporator, the throttle valve, the condenser, the auxiliary heat exchanger and a pipeline between the auxiliary heat exchanger and the main heat exchanger from the liquid nitrogen inlet pipeline;
the evaporator can utilize nitrogen entering from the main heat exchanger as a heat source for evaporating liquid oxygen, and simultaneously, the nitrogen is cooled into liquid nitrogen;
the condenser can utilize liquid nitrogen entering from the throttling valve as a cold source for condensing, evaporating and raising oxygen, and simultaneously evaporate the liquid nitrogen into nitrogen and enter the auxiliary heat exchanger.
The working principle and the beneficial effects are as follows: 1. the process is simple, oxygen (or liquid oxygen) discharged from the top of the krypton-xenon secondary concentration tower is sent into the cold box again through the buffer tank for rectification, and the preparation of high-purity oxygen can be realized only by arranging one rectification tower and a corresponding heat exchanger in the cold box;
2. the energy consumption is low, the nitrogen required in the process is recycled after being compressed by the nitrogen compressor, and the nitrogen and the oxygen can repeatedly recover cold and heat, so that the energy consumption is obviously reduced, the nitrogen emission is reduced, and the production cost is reduced;
3. the recovery rate of the high-purity oxygen is high and can reach more than 95 percent;
4. the device is completely independent of a krypton-xenon production system, does not share facilities such as a heat exchanger, avoids mutual influence when the working conditions of a high-purity oxygen system and the krypton-xenon production system fluctuate, and can be separated from the krypton-xenon production device to operate independently.
Further, the liquid nitrogen inlet pipeline is also communicated with a pipeline between the throttling valve and the condenser to be used as a liquid nitrogen supplementing pipeline. This arrangement is intended to sufficiently condense oxygen gas into liquid oxygen in the condenser.
Further, a vent is located between the main heat exchanger and the nitrogen compressor and before the nitrogen compressor. With the arrangement, part of redundant nitrogen gas can be discharged, excessive nitrogen gas in the liquid nitrogen circulation channel is prevented, and therefore liquid nitrogen is added into the liquid nitrogen circulation channel to supplement the nitrogen gas, so that part of nitrogen gas must be discharged.
A method for producing high purity oxygen based on the device for producing high purity oxygen comprises the following steps:
s1, introducing raw material oxygen into a main heat exchanger in a cold box from a buffer tank, introducing liquid nitrogen into a pipeline from the liquid nitrogen, cooling the raw material oxygen in the main heat exchanger to be partially liquefied by using nitrogen, reducing the pressure of the raw material oxygen, introducing the raw material oxygen into the middle upper part of a rectifying tower, heating the nitrogen in the main heat exchanger by using the raw material oxygen, emptying part of the nitrogen through an emptying pipe, and then introducing the nitrogen into a nitrogen compressor for compression;
s2, introducing the compressed nitrogen into the main heat exchanger for heat exchange, and then introducing the nitrogen into the evaporator as a heat source to evaporate liquid oxygen at the bottom of the rectifying tower into ascending steam, and cooling the nitrogen into liquid nitrogen;
s3, decompressing the liquid nitrogen through a throttle valve, enabling the liquid nitrogen to enter a condenser in a gas-liquid two-phase mode, synchronously introducing a strand of liquid nitrogen from a liquid nitrogen inlet pipeline as supplement, condensing the oxygen rising through evaporation into reflux liquid for rectification, enabling part of the rectified high-purity oxygen to enter an auxiliary heat exchanger, and enabling the liquid nitrogen to be evaporated into nitrogen and enter the auxiliary heat exchanger;
s4, in the auxiliary heat exchanger, the nitrogen and the liquid nitrogen simultaneously cool the high-purity oxygen gas into high-purity liquid oxygen, the high-purity liquid oxygen is extracted and discharged to a low-temperature storage tank for storage through a high-purity liquid oxygen outlet pipeline, and meanwhile, the nitrogen and the liquid nitrogen enter the main heat exchanger again for heat exchange;
s5, circularly executing the steps from S1 to S4, and continuously circularly purifying to produce high-purity liquid oxygen.
Utilize the method of this application to use the device of this application and make pure oxygen, possess the effect of device equally, simultaneously through cold volume and the heat of recycling nitrogen gas, effectively solved prior art and simply utilized the rectifying column to have the problem that the energy consumption is high, the ordinary oxygen that produces in the manufacturing process is not all useful moreover, also can become heat source or cold source, carries out the heat transfer with nitrogen gas, has reduced the waste, therefore the energy consumption is lower.
Further, in step S3, the oxygen gas that has been evaporated and risen enters the main heat exchanger to recover cold energy and is sent out of the cold box, and the remaining oxygen gas enters the condenser to be condensed into liquid oxygen by liquid nitrogen and is sent back to the top of the rectifying tower as reflux.
This step is further disclosed for recycling of oxygen.
The device for producing the high-purity oxygen comprises a liquid oxygen storage tank, a liquid nitrogen circulating channel and a cold box, wherein raw material liquid oxygen is arranged in the liquid oxygen storage tank; the cold box is internally provided with a main heat exchanger, a rectifying tower, an evaporator arranged at the bottom of the rectifying tower and a condenser arranged at the top of the rectifying tower;
the cold box is used for cooling all the components in the cold box so that all the components are at different temperatures, and the heat preservation is carried out among all the components by filling heat preservation materials;
the liquid oxygen storage tank is sequentially communicated with the rectifying tower and the main heat exchanger through a liquid oxygen channel, and high-purity liquid oxygen is discharged through a high-purity liquid oxygen outlet pipeline;
the liquid nitrogen circulation channel comprises a liquid nitrogen inlet pipeline positioned outside the cold box, a circulation pipeline partially positioned in the cold box, a vent pipe and a nitrogen compressor, wherein the vent pipe and the nitrogen compressor are positioned outside the cold box;
the evaporator can utilize nitrogen entering from the main heat exchanger as a heat source for evaporating liquid oxygen, and simultaneously, the nitrogen is cooled into liquid nitrogen;
the condenser can utilize the liquid nitrogen that gets into from the choke valve as the cold source of condensation evaporation rising oxygen, evaporates the liquid nitrogen for nitrogen gas simultaneously and gets into the main heat exchanger realization to the cyclic utilization of nitrogen gas.
The device has a similar structure and a basically consistent principle with the first device of the application, and the difference is that the raw material of the device is liquid oxygen, while the raw material of the first device is oxygen, and the two processing objects are different, but the device has the same advantages and the technical idea is consistent.
Further, the liquid nitrogen inlet pipeline is also communicated with a pipeline between the throttling valve and the condenser to be used as a liquid nitrogen supplementing pipeline. This arrangement is intended to sufficiently condense oxygen gas into liquid oxygen in the condenser.
Further, a vent is located between the main heat exchanger and the nitrogen compressor and before the nitrogen compressor. With the arrangement, part of redundant nitrogen gas can be discharged, and excessive nitrogen gas in the liquid nitrogen circulation channel is prevented, so that liquid nitrogen can be added into the liquid nitrogen circulation channel for supplement, and part of nitrogen gas must be discharged.
The method for producing high purity oxygen based on the device for producing high purity oxygen comprises the following steps:
s1, introducing raw material liquid oxygen from a liquid oxygen storage tank into the middle upper part of the rectifying tower, and introducing liquid nitrogen from a liquid nitrogen inlet pipeline;
s2, exchanging heat between the liquid oxygen and nitrogen passing through the evaporator at the bottom of the rectifying tower to evaporate the liquid oxygen into ascending steam;
s3, decompressing the liquid nitrogen through a throttle valve to form a gas-liquid two-phase mode, introducing a strand of liquid nitrogen from a liquid nitrogen inlet pipeline as supplement, condensing the oxygen ascending by evaporation into reflux liquid for rectification, sending the rest liquid oxygen to a main heat exchanger, evaporating the liquid nitrogen into nitrogen in the condenser, and extracting and discharging part of the rectified high-purity liquid oxygen through a high-purity liquid oxygen outlet pipeline;
s4, allowing the nitrogen and the liquid oxygen to enter a main heat exchanger for heat exchange and cold recovery, allowing the liquid oxygen to be discharged out of a cold box after cold recovery, allowing the nitrogen to be discharged into a part of nitrogen through a vent pipe after cold recovery, and allowing the rest of nitrogen to be sent into a nitrogen compressor for recycling;
s5, circularly executing the steps from S1 to S4, and continuously circularly purifying to produce high-purity liquid oxygen.
Utilize the method of this application to use the device of this application and make pure oxygen, possess the effect of device equally, simultaneously through cold volume and the heat of recycling nitrogen gas, effectively solved prior art and simply utilized the rectifying column to have the problem that the energy consumption is high, the ordinary oxygen that produces in the manufacturing process is not all useful moreover, also can become heat source or cold source, carries out the heat transfer with nitrogen gas, has reduced the waste, therefore the energy consumption is lower.
Further, the rectifying tower is a sieve plate tower or a packed tower.
Further, the nitrogen compressor compresses the nitrogen to 0.68MPa and then the nitrogen enters the main heat exchanger; the main heat exchanger exchanges heat with nitrogen and cools the nitrogen to below-173 ℃, and then the nitrogen enters the evaporator; the throttle valve decompresses the liquid nitrogen to 0.4Mpa, and then the liquid nitrogen enters the condenser in a gas-liquid two-phase mode.
Drawings
FIG. 1 is a schematic structural diagram of one embodiment of the present invention;
fig. 2 is a schematic structural diagram of another embodiment of the present invention.
In the figure, 1, a buffer tank; 2. a primary heat exchanger; 3. a rectifying tower; 4. an evaporator; 5. a condenser; 6. a secondary heat exchanger; 7. a nitrogen compressor; 8. cooling the box; 9. a throttle valve; 10. a liquid oxygen storage tank.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
It will be understood by those skilled in the art that in the present disclosure, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated in the drawings for ease of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, the above terms should not be construed as limiting the present invention.
In the case of the example 1, the following examples are given,
as shown in fig. 1, an apparatus for producing high purity oxygen comprises a buffer tank 1 in which a raw material oxygen is provided, a liquid nitrogen circulation passage, and a cold box 8; a main heat exchanger 2, a rectifying tower 3, an auxiliary heat exchanger 6, an evaporator 4 arranged at the bottom of the rectifying tower 3 and a condenser 5 arranged at the top of the rectifying tower 3 are arranged in the cold box 8;
the cold box 8 is used for cooling each part in the cold box 8 so that each part is at different temperatures, and heat preservation is carried out among the parts through filling heat preservation materials;
the buffer tank 1 is sequentially communicated with the main heat exchanger 2, the rectifying tower 3 and the auxiliary heat exchanger 6 through an oxygen channel, and high-purity liquid oxygen is discharged through a high-purity liquid oxygen outlet pipeline;
the liquid nitrogen circulation channel comprises a liquid nitrogen inlet pipeline positioned outside the cold box 8, a circulation pipeline partially positioned in the cold box 8, and an emptying pipe and a nitrogen compressor 7 positioned outside the cold box 8, wherein the circulation pipeline is sequentially communicated with the auxiliary heat exchanger 6, the main heat exchanger 2, the nitrogen compressor 7, the main heat exchanger 2, the evaporator 4, the throttle valve 9, the condenser 5, the auxiliary heat exchanger 6 and a pipeline between the auxiliary heat exchanger 6 and the main heat exchanger 2 from the liquid nitrogen inlet pipeline, the liquid nitrogen inlet pipeline is also communicated with the pipeline between the throttle valve 9 and the condenser 5 to serve as a liquid nitrogen supplementing pipeline, and the emptying pipe is positioned between the main heat exchanger 2 and the nitrogen compressor 7 and in front of the nitrogen compressor 7;
the evaporator 4 can use the nitrogen gas entering from the main heat exchanger 2 as a heat source for evaporating the liquid oxygen, and simultaneously cool the nitrogen gas into liquid nitrogen;
the condenser 5 can utilize liquid nitrogen entering from the throttle valve 9 as a cold source for condensing and evaporating ascending oxygen, and simultaneously, the liquid nitrogen is evaporated into nitrogen and enters the secondary heat exchanger 6.
The whole design is that on the basis of not influencing the original production of krypton and xenon, the rectifying tower 3, the main heat exchanger 2, the condenser 5/the evaporator 4 and the like are arranged in a single cold box 8, and oxygen (or liquid oxygen) discharged from the top of the krypton and xenon secondary concentration tower is sent into the cold box 8 again through the buffer tank 1 for rectification. The oxygen enters the upper part of a high-purity oxygen rectifying tower 3 after being cooled in a main heat exchanger 2 (if the oxygen is liquid oxygen, the oxygen directly enters the upper part of the high-purity oxygen rectifying tower 3, a condenser 5 is arranged at the top of the rectifying tower 3, and an evaporator 4 is arranged at the bottom of the tower.
The pressure nitrogen is cooled in the main heat exchanger 2 and then enters the bottom evaporator 4 of the high purity oxygen rectifying tower 3 to be used as a heat source, so that liquid oxygen in the rectifying tower 3 is evaporated to be ascending steam. Meanwhile, the nitrogen is condensed into liquid nitrogen, the liquid nitrogen is decompressed and then sent to a condenser 5 at the upper part of the rectifying tower 3 to be used as a cold source, steam rising from the top of the rectifying tower 3 is condensed into reflux liquid, the liquid nitrogen is evaporated into the nitrogen and then returns to the main heat exchanger 2 for reheating, and the nitrogen is compressed by a nitrogen compressor and then is recycled after being discharged from a cold box 8.
In the rectifying column 3, high purity oxygen (or liquid oxygen) having a purity of not less than 99.999% is extracted at the bottom of the column or at a position several trays apart from the bottom of the column. The position of the extraction opening is determined according to the content of high-boiling point components such as krypton, methane and the like in oxygen or liquid oxygen, and the extraction opening is preferably arranged at a plurality of tower plates away from the bottom of the tower, so that high-purity oxygen with higher purity can be obtained.
In the case of the example 2, the following examples are given,
based on the apparatus of example 1, example 2 is a method for producing high purity oxygen, comprising the steps of:
s1, introducing raw material oxygen into the main heat exchanger 2 in the cold box 8 from the buffer tank 1, introducing liquid nitrogen into a pipeline from the liquid nitrogen, cooling the raw material oxygen in the main heat exchanger 2 to be partially liquefied by using nitrogen, reducing the pressure of the raw material oxygen, introducing the liquefied raw material oxygen into the middle upper part of the rectifying tower 3, heating the nitrogen in the main heat exchanger 2 by using the raw material oxygen, emptying the partial nitrogen through an emptying pipe, and then introducing the partial nitrogen into the nitrogen compressor 7 for compression;
in this example and example 1, feed oxygen was 300Nm3H (0.24MPa, wherein the oxygen content is 99.7 percent, the nitrogen content is 2ppm, the argon content is 2700ppm, and the krypton and methane content are less than 1ppm), introducing the mixture into a main heat exchanger 2 in a cold box 8 from a buffer tank 1, cooling to be at least partially liquefied, and decompressing to enter the middle upper part of a rectifying tower 3.
S2, introducing the compressed nitrogen into the main heat exchanger 2 for heat exchange, and then allowing the nitrogen to enter the evaporator 4 as a heat source to evaporate liquid oxygen at the bottom of the rectifying tower 3 into ascending steam, and cooling the nitrogen into liquid nitrogen;
in this step, the evaporator 4 at the bottom of the rectifying column 3 is in the form of a plate-fin heat exchanger. 2000Nm3The nitrogen is compressed to 0.68MPa by a nitrogen compressor 7, enters a main heat exchanger 2 in a cold box 8, is cooled to minus 173 ℃ and then enters an evaporator 4 to be used as a heat source of the evaporator 4, so that the liquid oxygen at the bottom of the rectifying tower 3 is evaporated to be ascending steam, and the nitrogen is cooled to be liquid nitrogen in the evaporator 4.
S3, decompressing the liquid nitrogen through a throttle valve 9, enabling the liquid nitrogen to enter a condenser 5 in a gas-liquid two-phase mode, synchronously introducing a strand of liquid nitrogen from a liquid nitrogen inlet pipeline as supplement, condensing the oxygen rising by evaporation into reflux liquid for rectification, enabling part of the rectified high-purity oxygen to enter an auxiliary heat exchanger 6, and enabling the liquid nitrogen to be evaporated into nitrogen and enter the auxiliary heat exchanger 6;
in the step, the liquid nitrogen is decompressed to 0.4MPa through a throttle valve 9, enters a condenser 5 at the top of a rectifying tower 3 in a gas-liquid two-phase mode to be used as a cold source, and simultaneously a strand of liquid nitrogen (30 Nm & lt/EN & gt) is introduced from the outside of a cold box 83H) entering a condenser at the top of a rectifying tower 35, the oxygen gas rising in the rectifying tower 3 is condensed into reflux liquid by the liquid nitrogen and rectified.
Thus, the oxygen at the top of the rectifying tower 3 is divided into two parts, one part is sent to the main heat exchanger 2 to recover the cold energy and then sent out of the cold box 8; the other part enters a condenser 5 and is condensed into liquid oxygen by liquid nitrogen, and then the liquid oxygen is sent back to the top of the rectifying tower 3 to be used as reflux liquid.
S4, in the auxiliary heat exchanger 6, the nitrogen and the liquid nitrogen simultaneously cool the high-purity oxygen gas into high-purity liquid oxygen, the high-purity liquid oxygen is extracted and discharged to a low-temperature storage tank for storage through a high-purity liquid oxygen outlet pipeline, and meanwhile, the nitrogen and the liquid nitrogen enter the main heat exchanger 2 again for heat exchange;
in the step, after the liquid nitrogen is evaporated into nitrogen, the nitrogen enters the auxiliary heat exchanger 6 to recover part of cold energy, and a strand of liquid nitrogen (330 Nm & lt) is introduced from the outside of the cold box 83H) into the secondary heat exchanger 6, which two cold fluids are used to cool high purity oxygen gas having a purity of more than 99.999% to high purity liquid oxygen. High-purity oxygen is extracted from a plurality of tower plates above the bottom of the rectifying tower 3, and the flow rate is 292Nm3H, wherein the nitrogen content is less than 5ppm, the argon content is less than 2ppm, and the methane content is less than 0.5 ppm. The cooled liquid oxygen is sent out of the cold box 8 and enters a low-temperature storage tank for storage.
S5, circularly executing the steps from S1 to S4, and continuously circularly purifying to produce high-purity liquid oxygen.
In this embodiment, the rectifying column 3 can be a sieve tray column or a packed column, for example, a sieve tray column, on each tray, which provides a condition for sufficient contact between descending liquid and ascending vapor. Each contact of liquid with vapor is a process of both heat transfer and mass transfer. For each tray pass, the lower boiling components (argon, nitrogen, etc.) are reduced in the descending liquid while the higher boiling components (krypton, methane, etc.) are increased. After rectification by a certain number of tower plates, high-purity oxygen with the purity of more than 99.999 percent can be obtained at a plurality of tower plates above the bottom of the rectifying tower 3, liquid oxygen with relatively high boiling point components (krypton, methane and the like) is arranged at the bottom of the rectifying tower 3, and the high-purity oxygen can be safely discharged according to the content of methane in the components: e.g., -0.5 Nm3When discharging, the methane content in the liquid oxygen at the bottom of the rectifying tower 3 can be controlledAt 400 ppm.
In the case of the example 3, the following examples are given,
as shown in fig. 2, the present embodiment is different from embodiment 1 in that the processing object of the present embodiment is liquid nitrogen, and the apparatus for producing high purity oxygen includes a liquid oxygen storage tank 10 in which raw material liquid oxygen is provided, a liquid nitrogen circulation passage, and a cold box 8; a main heat exchanger 2, a rectifying tower 3, an evaporator 4 arranged at the bottom of the rectifying tower 3 and a condenser 5 arranged at the top of the rectifying tower 3 are arranged in the cold box 8;
the cold box 8 is used for cooling each part in the cold box 8 so that each part is at different temperatures, and heat preservation is carried out among the parts through filling heat preservation materials;
the liquid oxygen storage tank 10 is sequentially communicated with the rectifying tower 3 and the main heat exchanger 2 through a liquid oxygen channel, and high-purity liquid oxygen is discharged through a high-purity liquid oxygen outlet pipeline;
the liquid nitrogen circulation channel comprises a liquid nitrogen inlet pipeline positioned outside the cold box 8, a circulation pipeline partially positioned in the cold box 8, a vent pipe positioned outside the cold box 8 and a nitrogen compressor 7, wherein the circulation pipeline is sequentially communicated with the condenser 5, the main heat exchanger 2, the nitrogen compressor 7, the main heat exchanger 2, the evaporator 4, the throttle valve 9 and the condenser 5 from the liquid nitrogen inlet pipeline, the liquid nitrogen inlet pipeline is also communicated with a pipeline between the throttle valve 9 and the condenser 5 to serve as a liquid nitrogen supplementing pipeline, and the vent pipe is positioned between the main heat exchanger 2 and the nitrogen compressor 7 and in front of the nitrogen compressor 7;
the evaporator 4 can use the nitrogen gas entering from the main heat exchanger 2 as a heat source for evaporating the liquid oxygen, and simultaneously cool the nitrogen gas into liquid nitrogen;
the condenser 5 can utilize liquid nitrogen entering from the throttle valve 9 as a cold source for condensing, evaporating and rising oxygen, and simultaneously evaporate the liquid nitrogen into nitrogen and enter the main heat exchanger 2 to realize the cyclic utilization of the nitrogen.
The apparatus has a similar structure to that of the apparatus of example 1, and basically the same principle, except that the raw material of the apparatus is liquid oxygen, while the raw material of the apparatus of example 1 is oxygen, but the apparatus has the same advantages and the technical idea is the same. Therefore, the effects of the two are basically consistent.
In the case of the example 4, the following examples are given,
based on the apparatus of embodiment 3, the present embodiment is a method for producing high purity oxygen, comprising the steps of:
s1, introducing raw material liquid oxygen from the liquid oxygen storage tank 10 into the middle upper part of the rectifying tower 3, and introducing liquid nitrogen from a liquid nitrogen inlet pipeline;
in this example and example 3, the raw material liquid oxygen was 300Nm3H (0.24MPa, wherein the oxygen content is 99.7 percent, the nitrogen content is 2ppm, the argon content is 2700ppm, and the content of krypton and methane is less than 1ppm) is reduced in pressure from the liquid oxygen storage tank 10 and then led to the middle upper part of the rectifying tower 33.
S2, exchanging heat between the liquid oxygen and nitrogen passing through the evaporator 4 at the bottom of the rectifying tower 3 to evaporate the liquid oxygen into ascending steam;
2000Nm3the nitrogen is compressed to 0.68MPa by a nitrogen compressor 7, enters a main heat exchanger 2 in a cold box 8, is cooled to below-173 ℃, enters an evaporator 4 and is used as a heat source of the evaporator 4 of the rectifying tower 3, so that liquid oxygen at the bottom of the rectifying tower 3 is evaporated to form ascending steam, and the nitrogen is cooled to liquid nitrogen in the evaporator 4.
S3, decompressing the liquid nitrogen through a throttle valve 9, enabling the liquid nitrogen to enter a condenser 5 in a gas-liquid two-phase mode, synchronously introducing a strand of liquid nitrogen from a liquid nitrogen inlet pipeline as supplement, condensing the oxygen ascending by evaporation into reflux liquid for rectification, sending the rest liquid oxygen to a main heat exchanger 2, simultaneously evaporating the liquid nitrogen into nitrogen gas in the condenser 5, and extracting and discharging part of the rectified high-purity liquid oxygen through a high-purity liquid oxygen outlet pipeline;
the liquid nitrogen is decompressed to 0.4MPa by a throttle valve 9 and then enters a condenser 5 at the top of a rectifying tower 3 in a gas-liquid two-phase mode to be used as a cold source, and a strand of liquid nitrogen (63 Nm & lt/EN & gt) is introduced from the outside of a cold box 8 at the same time3And h) entering a condenser 5 at the top of the rectifying tower 3 for supplement, and condensing oxygen rising in the rectifying tower 3 into reflux liquid by the liquid nitrogen for rectification.
S4, allowing the nitrogen and the liquid oxygen to enter the main heat exchanger 2 for heat exchange and cold recovery, allowing the liquid oxygen to be discharged out of the cold box 8 after cold recovery, allowing the nitrogen to be discharged into a part of nitrogen through a vent pipe after cold recovery, and allowing the rest of nitrogen to be sent into the nitrogen compressor 7 for recycling;
wherein, the oxygen at the top of the rectifying tower 3 is divided into two parts, one part is sent to the main heat exchanger 2 to recover the cold energy and then sent out of the cold box 8; the other part enters a condenser 5 and is condensed into liquid oxygen by liquid nitrogen, and then the liquid oxygen is sent back to the top of the rectifying tower 3 to be used as reflux liquid.
S5, circularly executing the steps from S1 to S4, and continuously circularly purifying to produce high-purity liquid oxygen. High-purity liquid oxygen is extracted from a plurality of tower plates above the bottom of the rectifying tower 3, and the flow rate is-297 Nm3H, wherein the nitrogen content is < 5ppm, the argon content is < 2ppm and the methane content is < 0.5 ppm. The high-purity liquid oxygen is sent out of the cold box 8 and enters a low-temperature storage tank for storage.
The rectifying tower 3 is the same as that of the embodiments 1-2, and the present embodiment is the same as that of the embodiments 1 and 2 or adopts the same product with different specifications except that the auxiliary radiator and the buffer tank 1 in the embodiments 1 and 2 are not provided.
In summary, the main heat exchanger 2, the evaporator 4, the condenser 5, the rectifying tower 3, etc. described in examples 1 to 4, as well as the pipes, valves and various fluids flowing therein connecting these units are all at different low temperatures, and are installed in the cooling box 8, and the periphery of the cooling box 8 is spaced from all the containers and pipes to be filled with heat insulating material (e.g. expanded perlite) for insulating the low-temperature equipment.
The present invention is not described in detail in the prior art, and therefore, the present invention is not described in detail.
It is understood that the terms "a" and "an" should be interpreted as meaning that a number of one element or element is one in one embodiment, while a number of other elements is one in another embodiment, and the terms "a" and "an" should not be interpreted as limiting the number.
Although the terms buffer tank 1, main heat exchanger 2, rectifying column 3, evaporator 4, condenser 5, secondary heat exchanger 6, nitrogen compressor 7, cold box 8, throttle valve 9, liquid oxygen storage tank 10, etc. are used more herein, the possibility of using other terms is not excluded. These terms are used merely to more conveniently describe and explain the nature of the present invention; they are to be construed as being without limitation to any additional limitations that may be imposed by the spirit of the present invention.
The present invention is not limited to the above-mentioned preferred embodiments, and any other products in various forms can be obtained by anyone in the light of the present invention, but any changes in the shape or structure thereof, which have the same or similar technical solutions as the present application, fall within the protection scope of the present invention.

Claims (10)

1. A device for producing high-purity oxygen is characterized by comprising a buffer tank, a liquid nitrogen circulation channel and a cold box, wherein raw material oxygen is arranged in the buffer tank; the cold box is internally provided with a main heat exchanger, a rectifying tower, an auxiliary heat exchanger, an evaporator arranged at the bottom of the rectifying tower and a condenser arranged at the top of the rectifying tower;
the cold box is used for cooling all the components in the cold box so that all the components are at different temperatures, and the heat preservation is carried out among all the components by filling heat preservation materials;
the buffer tank is sequentially communicated with the main heat exchanger, the rectifying tower and the auxiliary heat exchanger through an oxygen channel, and high-purity liquid oxygen is discharged through a high-purity liquid oxygen outlet pipeline;
the liquid nitrogen circulation channel comprises a liquid nitrogen inlet pipeline positioned outside the cold box, a circulation pipeline partially positioned in the cold box, an emptying pipe and a nitrogen compressor, wherein the emptying pipe and the nitrogen compressor are positioned outside the cold box;
the evaporator can utilize nitrogen entering from the main heat exchanger as a heat source for evaporating liquid oxygen, and simultaneously, the nitrogen is cooled into liquid nitrogen;
the condenser can utilize liquid nitrogen entering from the throttling valve as a cold source for condensing, evaporating and raising oxygen, and simultaneously evaporate the liquid nitrogen into nitrogen gas to enter the auxiliary heat exchanger.
2. The apparatus for producing high purity oxygen in accordance with claim 1 wherein the liquid nitrogen inlet line is further in communication with a line between the throttling valve and the condenser as a liquid nitrogen make-up line.
3. The apparatus for producing high purity oxygen in accordance with claim 1 wherein the vent is located between the primary heat exchanger and the nitrogen compressor and before the nitrogen compressor.
4. A method for producing high purity oxygen, based on claim 3, wherein the apparatus for producing high purity oxygen comprises the steps of:
s1, introducing raw material oxygen into a main heat exchanger in a cold box from a buffer tank, introducing liquid nitrogen into a pipeline from the liquid nitrogen, cooling the raw material oxygen in the main heat exchanger to be partially liquefied by using nitrogen, reducing the pressure of the raw material oxygen, introducing the raw material oxygen into the middle upper part of a rectifying tower, heating the nitrogen in the main heat exchanger by using the raw material oxygen, emptying part of the nitrogen through an emptying pipe, and then introducing the nitrogen into a nitrogen compressor for compression;
s2, introducing the compressed nitrogen into the main heat exchanger for heat exchange, and then introducing the nitrogen into the evaporator as a heat source to evaporate liquid oxygen at the bottom of the rectifying tower into ascending steam, and cooling the nitrogen into liquid nitrogen;
s3, decompressing the liquid nitrogen through a throttle valve, enabling the liquid nitrogen to enter a condenser in a gas-liquid two-phase mode, synchronously introducing a strand of liquid nitrogen from a liquid nitrogen inlet pipeline as supplement, condensing the oxygen rising through evaporation into reflux liquid for rectification, enabling part of the rectified high-purity oxygen to enter an auxiliary heat exchanger, and enabling the liquid nitrogen to be evaporated into nitrogen and enter the auxiliary heat exchanger;
s4, in the auxiliary heat exchanger, the nitrogen and the liquid nitrogen simultaneously cool the high-purity oxygen gas into high-purity liquid oxygen, the high-purity liquid oxygen is extracted and discharged to a low-temperature storage tank for storage through a high-purity liquid oxygen outlet pipeline, and meanwhile, the nitrogen and the liquid nitrogen enter the main heat exchanger again for heat exchange;
s5, circularly executing the steps from S1 to S4, and continuously circularly purifying to produce high-purity liquid oxygen.
5. The method for producing high purity oxygen according to claim 4, wherein in step S3, the oxygen part rising through evaporation enters the main heat exchanger to recover cold and then is sent out of the cold box, and the rest part enters the condenser to be condensed into liquid oxygen by liquid nitrogen and then is sent back to the top of the rectifying tower as reflux liquid.
6. The device for producing high-purity oxygen is characterized by comprising a liquid oxygen storage tank, a liquid nitrogen circulating channel and a cold box, wherein raw material liquid oxygen is arranged in the liquid oxygen storage tank; the cold box is internally provided with a main heat exchanger, a rectifying tower, an evaporator arranged at the bottom of the rectifying tower and a condenser arranged at the top of the rectifying tower;
the cold box is used for cooling all the components in the cold box so that all the components are at different temperatures, and the heat preservation is carried out among all the components by filling heat preservation materials;
the liquid oxygen storage tank is sequentially communicated with the rectifying tower and the main heat exchanger through a liquid oxygen channel, and high-purity liquid oxygen is discharged through a high-purity liquid oxygen outlet pipeline;
the liquid nitrogen circulation channel comprises a liquid nitrogen inlet pipeline positioned outside the cold box, a circulation pipeline partially positioned in the cold box, a blow-down pipe positioned outside the cold box and a nitrogen compressor, and the circulation pipeline is sequentially communicated with the condenser, the main heat exchanger, the nitrogen compressor, the main heat exchanger, the evaporator, a throttle valve and the condenser from the liquid nitrogen inlet pipeline;
the evaporator can utilize nitrogen entering from the main heat exchanger as a heat source for evaporating liquid oxygen, and simultaneously, the nitrogen is cooled into liquid nitrogen;
the condenser can utilize the liquid nitrogen entering from the throttling valve as a cold source for condensing, evaporating and raising oxygen, and simultaneously evaporates the liquid nitrogen into nitrogen and enters the main heat exchanger to realize the cyclic utilization of the nitrogen.
7. The apparatus for producing high purity oxygen in accordance with claim 6 wherein the liquid nitrogen inlet line is further in communication with a line between the throttling valve and the condenser as a liquid nitrogen make-up line.
8. The apparatus for producing high purity oxygen in accordance with claim 7 wherein the vent is located between the primary heat exchanger and the nitrogen compressor and before the nitrogen compressor.
9. Method for producing high purity oxygen, characterized in that the apparatus for producing high purity oxygen according to claim 8 comprises the following steps:
s1, introducing raw material liquid oxygen from a liquid oxygen storage tank into the middle upper part of the rectifying tower, and introducing liquid nitrogen from a liquid nitrogen inlet pipeline;
s2, exchanging heat between the liquid oxygen and nitrogen passing through the evaporator at the bottom of the rectifying tower to evaporate the liquid oxygen into ascending steam;
s3, decompressing the liquid nitrogen through a throttle valve, enabling the liquid nitrogen to enter a condenser in a gas-liquid two-phase mode, synchronously introducing a strand of liquid nitrogen from a liquid nitrogen inlet pipeline as supplement, condensing the oxygen gas rising through evaporation into reflux liquid for rectification, sending the rest liquid oxygen to a main heat exchanger, meanwhile evaporating the liquid nitrogen into nitrogen gas in the condenser, and extracting and discharging part of the rectified high-purity liquid oxygen through a high-purity liquid oxygen outlet pipeline;
s4, allowing the nitrogen and the liquid oxygen to enter a main heat exchanger for heat exchange and cold recovery, allowing the liquid oxygen to be discharged out of a cold box after cold recovery, allowing the nitrogen to be discharged into a part of nitrogen through a vent pipe after cold recovery, and allowing the rest of nitrogen to be sent into a nitrogen compressor for recycling;
s5, circularly executing the steps from S1 to S4, and continuously circularly purifying to produce high-purity liquid oxygen.
10. The method for producing high purity oxygen in accordance with claim 9, wherein the nitrogen compressor compresses the nitrogen to 0.68MPa and then feeds the compressed nitrogen into the main heat exchanger; the main heat exchanger exchanges heat with nitrogen and cools the nitrogen to below-173 ℃, and then the nitrogen enters the evaporator; the throttle valve decompresses the liquid nitrogen to 0.4Mpa, and then the liquid nitrogen enters the condenser in a gas-liquid two-phase mode.
CN202210093413.3A 2022-01-26 2022-01-26 Device and method for producing high-purity oxygen Active CN114440554B (en)

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